2-Piperidinecarboxylic acid, 2-Methyl-, Methyl ester synthesis

Yield:-

Reaction Conditions:

with hydrogenchloride in dichloromethane;ethyl acetate; for 0.333333 h;

Steps:

(2-Methylpiperidin-2-yl)methanol

Methyl N-Boc-2-methylpiperidine-2-carboxylate (5.0g,19.45mmol) was dissolved in dichloromethane (15mL),Hydrogen chloride ethyl acetate solution (30 mL) was added,and the reaction solution was concentrated after 20 minutes. Add dichloromethane (20 mL) and sodium carbonate solid to adjust the pH to 7-8. Filtration and concentration of the filtrate gave the crude product of methyl 2-methylpiperidine-2-carboxylate,which was dissolved in tetrahydrofuran (20 mL). This solution was added dropwise to a solution of lithium aluminum hydride in tetrahydrofuran (30 mL,23.3 mmol) at 0°C,stirred at 0°C for 2 hours,quenched by sodium sulfate decahydrate,stirred at room temperature for 30 minutes,filtered,and the filtrate was concentrated to obtain the title compound (1.8 g,72%).

References:

CN112778331,2021,A Location in patent:Paragraph 0321-0324